Process of producing a dispersive agent



Pat'ented Aug. 14, 1945 annuis. Tiede, Detroit, ich, assignor to v firover (1. Bear, Detroit, Mich.

I No Drawing. Application March 10, 1942,

Serial No. 434,122

2 Glaims.

' This invention relates to dispersive agents and particularly agents inducing gaseous dispersions in liquid or semi-liquid mediums, and further relates to extraction of such agents from vegetable matter and treatment of the extract to increase its dispersive efiect, eliminate toxicity, if any and reduce theproduct to a readily marketable form.

Gaseous dispersions have various well-known uses'as for example, the reduction of sugar or starch solutions, gums or gelatines to an aerated and expanded -form for imparting lightness and volume to food products. Considerable stability or permanency is often desirable for such expanded products, and to promote these characteristics and further improve the appearance of said products, it is desirable that the dis ersed gas cells or globules be of uniformly small cell structure. I

An object of the invention is to provide an agen highly conducive to a. agseous dispersion in water and in various other lqiuid or semi-liquid mediums, and imparting a much greater degree of stability than has been heretofore attained for such dispersions. V

A further object is to provide an agent suited to induce a gaseous dispersion in liquid mediums and to achieve a marked increase in uniformity of dispersed globules, as compared to prior practice.

plant materials such saponin as is present. After filtering oil or otherwise removing the alcoholic extract, the plant materials are washed and then subjected to a further and exhaustive extraction, using moderately alkaline water as the extractive medium; said materials being preferably previously soaked in such water for a period of fifteen hours or more. 'Iioimpart desired alkalinity, the water may be treated with any of various alkalis, as for example, sodium borate, hydroxide,

' or ammonium hydroxide. i The purpose of alkalinity is to destroy enzymes extracted from the plant material, and to replace such enzymes with others of nontoxic'nature there is further added to the water a suitable quantity of cereal gluten. Also it is preferred to add a sufficient quality of pure tea at this time to counteract toxicity. After heating the plant materials andtreated water almost to the boiling point, the extract is filtered under vacuum, I syrup. This syrup is now treated, while boiling,

A further object is to derive the desired agent by extraction from vegetable matter containing cam ing and to avoid contamination of the agent by such glucosldes.

While the variety of plants from which desired dispersive agent may be extracted is quite large, those considered most available and best suited to the purpose are as follows: Saponaria o'fllcinatis, Aarostemma cithago, Sapindus saponaria, Gypsophiliu. struthium, Quillaia saponaria, Polygala sencga, Monimid polystacnia, Chrysophyllum glycvphleum and syringa These it will be noted are oil and concentrated by evaporation, preferably being; thus reduced to a heavy with an aqueous solution of a suitable catalyst, as zinc chloride or is purified with lead acetate. The liquid is now filtered and the filtrate is allowed to cool and is treated with either acetone or ether, in equal amount. There results a' finely divided precipitate from which the liquid may be filtered or drawn oil. To further purify this precipitate it is rewashed with acetone, ether, or alcohol and it may be further treated with chloroform to remove coloring matter, if present. Finally, the precipitate is dried, preferably under vacuum and in presence of carbon dioxide, its final form being that of a very light, chain and readily soluble powder.

Following is a more concise statement of the process, with definite weights given for materials saponin-yieldin'g plants and one of the features of present invention is elimination of saponin from desired product. Qapcnin has been used to some t extent to produce foam or froth in beverage maniifacture, but it is undesirable for my purpose due to its toxicity and because I have discovered a more effective agent.

One or more of the plants identified or selected portions thereof, are chopped, crushed, powdered, or otherwise prepared for extraction. An initial extraction from the materials thus prepared is accomplished by treating them with ethyl or methyl alcohol or both, preferably byboiling the alcohol under suitable pressure. The purpose of this initial extraction is to withdraw from the employed. I 1b 120 cc. of ethyl or methyl alcohol or a mixture thereof add 2 cc. of ammonium water, U. S. P.

from 27% to 29%, and 22 grams of suitably prepared Quillada bark. Allow to soak for twelve hours or more and then heat almost to boiling point. Separate the resulting extract from the bark by filtration or in other suitable manner. Place the residual bark in 300 cc. of cold water wherein /2 gram of sodium bore-ta has been dissolved, together with 3 grams of processed gluten and 1% grams of pure tea. After hie-sting the liquid almost to the boiling poini add 0.2 gram of zinc chloride or lead acetate. Again heat almost to boiling point, then strain or filter. Add

to residue cc. of water, heat as before, strain.

and filter. and add resulting filtrate to that obteined earlier in the process. Evcpomte-until a thick syrup remains and allow to cool. Trout this syrup with an equal volume of ecetoue to dissolve its soluble ingredients including the met- 2.] salt or salts. Filter 0-13 or otherwise withdrew the liquid. Rewesh the residue with edditiomel acetone or alcohol, and such residue when: dried will bee, light chalky powder. It necessely to remove coloring matter, treatment-oi residue with chloroform will serve that purpose.

Product thus attained is highly eiiective es s. dispersive agent, particularly for inducing g%' ous dispersions. Thus, for example, if u. crew c2 this powder isedded to 120 cc. 0! water OE other suitable liquid and such liquid is thoroughly cei= teted, as by a. power heating mechanism, the limuid becomes highly aerated and expended, due to dispersion therein of smell uniform elohulee of air characterized by a. much greater stability than hes been heretofore attained. In the case of a complete dispersion, or one comprised en= tirely of globules, this stability is such that the mass may be cut into slices like u, solid, without materiel resulting transition to liquid ileum. its further indicating the very considerable dioces sive efiect of the agent produced so ehove ele= scribed, it may he mentioned that it will so hereto 2. given volume of water as to multiply tlzslt' yol= ume approximately twenty-four times.

There are many uses for the dispersive agent produced as described. since inclusion oi any toiuc ingredient 22% been avoided, it is iecsihle to use the agent in many foods and beverages where lasting aerating effect is desired. Such on effect is further sometimes desiruble in other products es seeps, dyes, plant foods and plastics.

As a icy-product of the process decci'iheil, seponin may be recovered from the extinct formed by the initial or alcoholic treatment of the plant materials. Thus the alcoholic extract may be evaporated, by heating or evacuation or both, until it is reduced to a. thick syrup. If it is desired to destroy or counteract toxicity in the scpcuin, the syrup may now be treated with s. concentrated tee extract or with any of the following: cholesterol, acetic euhydrate, uutreotecl lecithin, or ergosterol. ilineily, the W is treated with ecetoue or other to dmsolve all imeredichts other then theseponin. Alter separating the letter from the liquid, it is washed with coiditiouel acetone or ether and upon drying it essumes the form of u very fine and light chalky powder.

What I clelm is:

i. A process of producing a. dispersive agent, which comprises comminutmg to e finely divided fiorm coconut-containing vegetable matter prepemtcry to extraction, subjecting said matter for extraction purcoses to methyl alcohol as 9, s01- vezit, separating the extract from the vegetable residue, treating such residue with alkaline water to efiect e. iurther extraction and destroy enwmes, adding at suitelole quantity of cereal gluten to replace such enzymes, heating the treated residue to on epproximcte boiling temperature, sepstating the resultant emrect from the residue,

concentrating thexextrect to syrup consistency,

boiling the concentrate and treating it while boillog with clue chloride in equeous solution as a. cctclyst, filtering the product and treating the iiitircte, when cooled, with ucetone to obtain a, precipitate, separating the precipitate from the illtmte. Washing it with acetone, and drying such precipitate.

2. A process of producing e. dispersive agent, which compi'iees commlnutlng to it finely divided iox iu sc eme-containing vegetable matter prepsretory to extraction, subjecting said matter for extrectiou purposes to methyl alcohol as 8. s01- veut, concreting the extract from the vegetable reeiciue, treating such residue with alkaline water to effect further extraction and destroy, enzymc', cclchug o. suitable quantity of cereal gluten to replace such enzymes and also adding substcutiully pure tee. to counteract toxicity, heatin the treated residue to an approximate boiling temperature, separating the resultant extract from the residue, concentrating the extract to syrup consistency, boiling the concentrate and tiieutihg it while coiling with zinc chloride in aqueous solution as c. catalyst, filtering the product cud treating the filtrate, when cooled, with ccetoue to obtain s precipitate, separating the precipitate from the filtrate, washing it with acetone, sud drying such precipitate..

AJRTEUR J. mu. 

